CN102105610B - Copper alloy sheet material and manufacturing method thereof - Google Patents
Copper alloy sheet material and manufacturing method thereof Download PDFInfo
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- CN102105610B CN102105610B CN200980128877.6A CN200980128877A CN102105610B CN 102105610 B CN102105610 B CN 102105610B CN 200980128877 A CN200980128877 A CN 200980128877A CN 102105610 B CN102105610 B CN 102105610B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/10—Alloys based on copper with silicon as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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Abstract
Disclosed is a copper alloy sheet material that has a composition containing Ni and/or Co at a total content of 0.5-5.0 mass%, 0.3-1.5 mass% Si, and the remainder copper as well as unavoidable impurities, and wherein the surface area percentage of cube orientation {0 0 1} is 5-50% with crystal orientation analysis using EBSD measurement.
Description
Technical field
The present invention relates to a kind of copper alloy plate and manufacture method thereof that is applied to lead frame, junctor, terminal material, rly., switch and socket etc. that electric/electronic device uses.
Background technology
The desired characteristic item of Cu alloy material that is used for the electric/electronic device purposes such as lead frame, junctor, terminal material, rly., switch and socket has electric conductivity, endurance (yield stress), tensile strength, bendability and stress relaxation-resistant characteristic.In recent years, along with the high temperature of miniaturization, lightweight, multifunction, high-density installation and the environment for use of electric/electronic device, this requires characteristic also to uprise.
At present, as common electric/electronic device material, except ferrous material, the copper based material of phosphor bronze, red copper and brass etc. also is being widely used.These alloys have improved intensity by the combination by the cold worked work hardening of the solution strengthening of Sn or Zn and rolling, wire drawing etc.In the method, electric conductivity is not enough, in addition, owing to obtain high strength by applying high cold working rate, thereby bendability and stress relaxation-resistant characteristic deficiency.
Instead the reinforcement of aforesaid method has the precipitation strength that makes trickle Second Phase Precipitation in material.This enhancement method is owing to specifically also improving the advantage of electric conductivity, so all adopt in a lot of alloy series when intensity uprises.Wherein, the Cu-Ni-Si that makes the compound of Ni and Si separate out minutely reinforcement in Cu is that the alloy C70250 of CDA " Copper Development Association: copper development association " registration alloy (for example, as) has the high advantage of the ability of its reinforcement and is widely used.In addition, especially with Co replaced Ni part or all Cu-Ni-Co-Si system or Cu-Co-Si be alloy to have than Cu-Ni-Si be the higher advantage of electric conductivity, thereby be used in the purposes of a part.But, along with the miniaturization of recent electronics, the employed parts of automobile, the copper alloy that is used becomes more high-intensity material is applied the state of bending machining with minor radius more, thus the copper alloy plate of demand bendability brilliance consumingly.Although in existing Cu-Ni-Co-Si is, in order to obtain high strength, obtained larger work hardening by improving Reduction by rolling, the method can cause bendability to worsen as mentioned above, fails to take into account high strength and good bendability.
For the requirement of described raising bendability, some schemes that solve by the control crystalline orientation have been proposed.In patent documentation 1, find that the Cu-Ni-Si series copper alloy is at crystal grain diameter with from { 311}, { 220}, { X-ray diffraction intensity of 200} face satisfies in the situation of crystalline orientation of certain condition and has excellent bendability.In addition, in patent documentation 2, find that the Cu-Ni-Si series copper alloy is from { 200} face and { X-ray diffraction intensity of 220} face satisfies in the situation of crystalline orientation of certain condition and has excellent bendability.In addition, in patent documentation 3, find the Cu-Ni-Si series copper alloy by control cube orientation 100}＜001〉and the bendability of ratio with excellence.
Patent documentation 1: TOHKEMY 2006-009137 communique
Patent documentation 2: TOHKEMY 2008-013836 communique
Patent documentation 3: TOHKEMY 2006-283059 communique
Summary of the invention
The problem that invention will solve
But, in the invention that patent documentation 1 or patent documentation 2 are put down in writing, relevant { 200}, { 220} and the { information of the minimum part of the analysis of the assembly of the limited specific crystal plane such as 311} during only wide crystal plane distributes.And, nothing but the crystal plane of only having measured plate face direction, about which crystal plane towards rolling direction or plate width direction, disclose.Therefore, the summary of the invention of putting down in writing based on patent documentation 1 or patent documentation 2 is controlled the set tissue of excellent in bending workability, and is sometimes thorough not, abundant not.In addition, in the invention that patent documentation 3 is put down in writing, the control of crystalline orientation realizes by the Reduction by rolling that reduces after the solutionizing thermal treatment.
On the other hand, along with in recent years more and more miniaturization of electric/electronic device, multifunction, high density packing etc., the Cu alloy material that is used for electric/electronic device also is required to have the bendability higher bendability more contemplated than the invention of putting down in writing at above-mentioned each patent documentation.
In view of above situation, the technical problem to be solved in the present invention is, the copper alloy plate that is suitable for lead frame that electric/electronic device uses, junctor, terminal material etc. and the automobile mounted junctor of using etc. or terminal material, rly., switch etc. that a kind of bendability is remarkable and have remarkable intensity is provided.
For the means of dealing with problems
The present application people is studied the copper alloy that is suitable for the electrical and electronic parts purposes, and in the copper alloy of Cu-Ni-Si system, Cu-Ni-Co-Si system, Cu-Co-Si system, in order greatly to improve bendability, intensity, electroconductibility, stress relaxation characteristics, find cube orientation assembly ratio and especially the ratio of S orientation is relevant with bendability, and finally finished the present invention through wholwe-hearted research.In addition, on this basis, also in this alloy system, having the electric conductivity do not damaged and bendability and improving intensity and the interpolation element of the function of stress relaxation characteristics is invented.In addition, invented the manufacture method that is used for realizing crystalline orientation as described above.
According to the present invention, can provide following means:
(1) a kind of copper alloy plate, it is characterized in that, has following composition: comprise any a kind or 2 kinds among Ni that total amount is 0.5～5.0mass% and the Co, and comprise the Si of 0.3～1.5mass%, and remainder is comprised of copper and inevitable impurity, in the crystalline orientation that utilizes EBSD to measure is analyzed, the cube orientation 001}＜100〉and area occupation ratio be 5～50%;
(2) a kind of copper alloy plate, it is characterized in that, has following composition: comprise any a kind or 2 kinds among Ni that total amount is 0.5～5.0mass% and the Co, and comprise the Si of 0.3～1.5mass%, and remainder is made of copper and inevitable impurity, in the crystalline orientation that utilizes EBSD to measure is analyzed, the cube orientation 001}＜100〉and area occupation ratio be 5～50%, S orientation 231}＜346〉and area occupation ratio be 5～40%;
(3) according to above-mentioned (1) or (a 2) described copper alloy plate, it is characterized in that, described copper alloy comprise total amount be 0.005～1.0mass% from the group who is formed by Sn, Zn, Ag, Mn, B, P, Mg, Cr, Fe, Ti, Zr and Hf, select at least a;
(4) according to each described copper alloy plate in above-mentioned (1) to (3), it is characterized in that, the Cube orientation 001}＜100〉and the average crystal grain diameter of crystal grain be less than or equal to 20 μ m;
(5) a kind of manufacture method of copper alloy plate, it is characterized in that, for the manufacture of each described copper alloy plate in the item of above-mentioned (1) to (4), wherein, become described copper alloy plate raw material the copper alloy starting material by the casting [operation 1], thermal treatment [operation 2] homogenizes, hot-work [operation 3], water cooling [operation 4], cutting [operation 5], cold rolling [operation 6], thermal treatment [operation 7], cold rolling [operation 8], middle solutionizing thermal treatment [operation 9], cold rolling [operation 10], Precipitation thermal treatment [operation 11], the order of precision work cold rolling [operation 12] and modified annealing [operation 13] is implemented to process, described thermal treatment [operation 7] is 400～800 ℃ temperature, carry out in 5 seconds～20 hours the scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, with the working modulus R2's (%) in the working modulus R1 (%) in the described cold rolling [operation 10] and the described precision work cold rolling [operation 12] be made as 5～65%;
(6) according to the manufacture method of above-mentioned (5) described copper alloy plate, it is characterized in that, with described Precipitation thermal treatment [operation 11] as finishing operation, described thermal treatment [operation 7] is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, and the working modulus R1 (%) in the described cold rolling [operation 10] is made as 5～65%;
(7) according to the manufacture method of above-mentioned (5) described copper alloy plate, it is characterized in that, implement described Precipitation thermal treatment [operation 11] as the subsequent processing of solutionizing thermal treatment [operation 9] in the middle of described, described thermal treatment [operation 7] is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, and the working modulus R2 (%) in the described precision work cold rolling [operation 12] is made as 5～65%;
(8) according to the manufacture method of above-mentioned (5) described copper alloy plate, it is characterized in that, implement described cutting [operation 5] as the subsequent processing of described hot-work [operation 3], described thermal treatment [operation 7] is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, with the working modulus R2's (%) in the working modulus R1 (%) in the described cold rolling [operation 10] and the described precision work cold rolling [operation 12] be made as 5～65%; And
(9) according to the manufacture method of above-mentioned (5) described copper alloy plate, it is characterized in that, implement described hot-work [operation 3] as the subsequent processing of described casting [operation 1], described thermal treatment [operation 7] is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, with the working modulus R2's (%) in the working modulus R1 (%) in the described cold rolling [operation 10] and the described precision work cold rolling [operation 12] be made as 5～65%.
The invention effect
According to the present invention, can provide the copper alloy plate that is suitable for the electric/electronic device purposes of each excellent of intensity, bendability, electric conductivity, stress relaxation-resistant characteristic.
Above-mentioned and other feature and the advantage content of reading following record by the accompanying accompanying drawing of suitable reference of the present invention will be more readily apparent from.
Description of drawings
Figure 1A, Figure 1B are the explanatory views of the test method of stress relaxation characteristics, and wherein, Figure 1A shows the state before the thermal treatment, and Figure 1B shows the state after the thermal treatment.
Fig. 2 is based on the explanatory view of the stress relaxation test method of JCBA T309:2001 (temporarily).
Description of reference numerals
1 test piece when having applied initial stress
2 remove the test piece behind the load
The 3 not test pieces during loading stress
4 testing tables
11 test pieces (during unloading)
12 test piece anchor clamps
13 reference planes
14 are used for loading the screw of deflection
15 test pieces (when loading deflection)
Embodiment
Preferred implementation to copper alloy plate of the present invention is elaborated.In addition, " sheet material " among the present invention also comprises " web ".
In the present invention, by nickel (Ni), cobalt (Co) and silicon (Si) separately the addition of control to the middle interpolation of copper (Cu), the compound of Ni-Si, Co-Si, Ni-Co-Si is separated out (precipitation), thereby improve the intensity of copper alloy.It is 0.5～5.0mass% that copper alloy among the present invention comprises total amount, be preferably 1.0～4.0mass%, more preferably Ni and the Co of 1.5～3.5mass%.Both can only contain among Ni and the Co any, also can contain two kinds of Ni and Co.The content of Ni is preferably 0.5～4.0mass%, 1.0～4.0mass more preferably, and the content of Co is preferably 0.5～2.0mass%, more preferably 0.6～1.7mass.In addition, the copper alloy among the present invention comprise 0.3～1.5mass%, be preferably 0.4～1.2mass%, the Si of 0.5～1.0mass more preferably.If the addition of Ni, Co, Si is too much, will cause electric conductivity to descend, in addition, if when very few, then intensity is just not.
In order to improve the bendability of copper alloy plate, the present application people investigates the generation reason of the crackle that produces in bending machining section.Its result, confirmed that reason is: viscous deformation is local to be enlarged, thereby forms the shearing strain band, and owing to local work hardening has caused generation and the connection of micropore, thereby reach forming limit.As its countermeasure, recognize that raising difficulty in flexural deformation causes that the ratio of the crystalline orientation of work hardening is resultful.That is to say, invented cube orientation 001}＜100〉and area occupation ratio demonstrate good bendability when being 5%～50%.If the area occupation ratio of cube orientation is less than 5%, then its effect is inadequate.In addition, as want than 50% higher, then must carry out cold rolling processing after recrystallize is processed with low working modulus, intensity obviously reduces, so not preferred.In addition, if be higher than 50%, stress relaxation characteristics also can descend, so not preferred.Preferred scope is 7～47%, more preferably 10～45%.
In addition, the method for expressing of the crystalline orientation in this specification sheets adopts the rolling direction (RD) of material to get X-axis, plate width direction (TD) and gets the rectangular coordinate system that Y-axis, rolling normal direction (ND) are got Z axis, and each zone in the material is used with the formation with (h k l) [u v w] of the index [u v w] in the index (hkl) of vertical (parallel with the rolling surface) crystal face of Z axis and the crystal orientation parallel with X-axis and represented.In addition, as (132) [6-43] and (231) [3-46] etc., about the orientation of equivalence on the symmetry basis of the cubic system of copper alloy, use the bracket symbol of expression family, be expressed as h k l}＜u v w.Cube orientation with 001}＜100〉and exponential representation, the S orientation with 231}＜346〉and exponential representation.
In addition, on the cube of above-mentioned scope orientation basis, preferably exist 5～40% scope the S orientation 231}＜346〉because this is conducive to improve bendability.S orientation 231}＜346〉area occupation ratio more preferably 7%～37%, more preferably 10%～35%.Except cube orientation and S orientation, also can produce Copper orientation 121}＜1-11 〉, the D orientation 4114}＜11-811 〉, the Brass orientation 110}＜1-12 〉, the Goss orientation 110}＜001 〉, the R1 orientation 236}＜385〉etc., if but cube is orientated the area occupation ratio with 5～50%, the area occupation ratio that S is orientated with 5～40% exists, and then allows to comprise these orientation components.
The analysis and utilization in the above-mentioned crystal orientation among the present invention the EBSD method.The EBSD method is the abbreviation of Electron Back-Scatter Diffraction (electron backscattered analysis), is the crystal orientation analytical technology of having utilized the Kikuchi lines reflection electron diffraction that produces in scanning electronic microscope (SEM) when test portion shines electric wire.For 0.1 micron that comprises 200 above crystal grain square test portion area, scan with 0.5 micron etc. stride, and analyzed orientation.Measure area and scan stride and adjust according to the size of the crystal grain of test portion.Area occupation ratio of each orientation is ratio with respect to whole mensuration area, described whole mensuration area be with respect to the cube orientation 001}＜100〉and the S orientation 231}＜346〉ideal orientation at ± 10 ° with interior area.Although the information that obtains in the orientation analysis that has utilized the EBSD method comprises that electric wire invades test portion until the orientation information of tens nm depths, since very little than the area of measuring, therefore be designated as in this manual area occupation ratio.In addition, the surface part of slave plate is measured.
In the analysis in crystal orientation, by using EBSD to measure, very differently can obtain with high resolving power the complete crystal orientation information of three-dimensional with the mensuration of gathering of the specific atoms face that plate face direction was carried out by X-ray diffraction method in the past, therefore about the crystal orientation of control bendability, can obtain brand-new information.
Then, the effect of adding element to the pair of this alloy interpolation is shown.As the preferred secondary element that adds, can enumerate: Sn, Zn, Ag, Mn, B, P, Mg, Cr, Fe, Ti, Zr and Hf.It is not preferred that the total amount of these elements surpasses 1mass%, because in case above 1mass%, will produce the drawback that electric conductivity descends.When adding secondary interpolation element, in order fully to effectively utilize additive effect and electric conductivity to be descended, secondary total amount of adding element need to be 0.005～1.0mass%, is preferably 0.01mass%～0.9mass%, more preferably 0.03mass%～0.8mass%.The additive effect of each element below is shown.
Mg, Sn, Zn improve the stress relaxation-resistant characteristic by adding in Cu-Ni-Si system, Cu-Ni-Co-Si system, the Cu-Co-Si series copper alloy.Compare when adding separately respectively, when adding simultaneously, by the synergism effect, can further improve the stress relaxation-resistant characteristic.In addition, be significantly improved the welding embrittlement effect.
If add Mn, Ag, B, P, then can improve hot workability, and improve intensity.
Cr, Fe, Ti, Zr, Hf with separate out minutely as main Ni, the Co of element and the compound of Si or the form of monomer of adding, help precipitation-hardening.In addition, as compound, separate out by the size with 50～500nm, suppress grain growing, make crystal grain diameter become small effect thereby have, and make bendability become good.
In addition, the average crystal grain diameter of the crystal grain of cube orientation is preferably less than or equal to 20 μ m, more preferably less than or equal to 17 μ m, and 15～3 μ m more preferably.Be controlled in the above-mentioned scope by the average crystal grain diameter with the crystal grain of cube orientation, the effect that reduces the wrinkle that produce on the bend surface is arranged, can realize more remarkable bendability.The average crystal grain diameter of the crystal grain of the cube orientation among the present invention is the following value of calculating: in the orientation analysis that has utilized above-mentioned EBSD method, only extract the zone that the cube orientation is shown and measure crystal grain diameter, and calculate as mean value.In addition, in the case, as with the twin crystal orientation of the cube orientation of cube orientation adjacency 221}＜212〉orientation is included in and carried out the value of analyzing in the cube orientation.
Then, preferably creating conditions of copper alloy plate of the present invention described.In an example of the manufacture method of existing precipitation type copper alloy, casting [operation 1] copper alloy starting material, obtain ingot bar, with its thermal treatment that homogenizes [operation 2], and carry out thin plate by the order of the hot-work such as hot rolling [operation 3], water-cooled [operation 4], cutting [operation 5], cold rolling [operation 6], in the temperature range of 700～1020 ℃ of temperature, carry out centre solutionizing thermal treatment [operation 9] solute atoms is dissolved again, the intensity of then satisfying the demand by Precipitation thermal treatment [operation 11] and precision work cold rolling [operation 12].In this a series of operation, the set tissue of material is roughly determined by the recrystallize that causes in middle solutionizing thermal treatment, and is finally determined by the rotation that causes in precision work is rolling.
In the preferred implementation of the manufacture method of copper alloy plate of the present invention, by being increased in before the thermal treatment [operation 7] carried out in 400 ℃～800 ℃ temperature, 5 seconds～20 hours the scope in this centre solutionizing thermal treatment [operation 9] and less than or equal to the cold rolling [operation 8] of 50% working modulus, in the recrystallize set tissue in middle solutionizing thermal treatment [operation 9], the area occupation ratio of cube orientation increases.Here, thermal treatment [operation 7] is compared with middle solutionizing thermal treatment [operation 9], carries out with low temperature., in thermal treatment [operation 7] and middle solutionizing thermal treatment [operation 9], carry out long thermal treatment during preferred low temperature here, carry out the thermal treatment of short period of time during high temperature.
If the treatment temp during thermal treatment [operation 7] is lower than 400 ℃, the tendency of recrystallize does not strengthen, and is therefore not preferred.If treatment temp is higher than 800 ℃, the tendency that the crystal grain diameter chap is large strengthens, and is therefore not preferred.Therefore, preferred 450～750 ℃ of the treatment temp of thermal treatment [operation 7], further preferred 500～700 ℃.In addition, preferred 1 minute～10 hours of the treatment time of thermal treatment [operation 7], further preferred 30 minutes～4 hours.In the relation of the temperature and time of thermal treatment [operation 7], preferred 1 minute～10 hours of the treatment time during 450～750 ℃ of temperature (is long-time during low temperature, be the short period of time during high temperature), preferred 30 minutes～4 hours for the treatment of time when treatment temp is 500～700 ℃ (for long-time, being the short period of time during high temperature during low temperature).The working modulus of cold rolling [operation 8] is preferably less than or equal to 45%, and further preferred 5～40%.In addition, preferred 750～1020 ℃ of the treatment temp of middle solutionizing thermal treatment [operation 9], preferred 5 seconds～1 hour for the treatment of time.
In addition, after middle solutionizing thermal treatment [operation 9], implement cold rolling [operation 10], Precipitation thermal treatment [operation 11], precision work cold rolling [operation 12] and modified annealing [operation 13].Here, preferably carry out take cold rolling [operation 10] and precision work cold rolling [operation 12] working modulus R1 separately and the summation of R2 as 5～65% working modulus.Under the working modulus below 5%, the work hardening amount is few, insufficient strength, under the working modulus more than 65%, the cube orientation area that generates in middle solutionizing thermal treatment is because of other orientations such as the rolling Copper of rotating to is orientated, D orientation, S orientation, Brass orientations, thereby the area occupation ratio of cube orientation descends, and is therefore not preferred.The summation of working modulus R1 and R2 more preferably 10～50%.In addition, following calculating processing rate R1 and R2.
R1(％)＝(t[9]-t[10])/t[9]×100
R2(％)＝(t[10]-t[12])/t[10]×100
Here, t[9], t[10], t[12] be respectively in the middle of after solutionizing thermal treatment [operation 9], the thickness of slab behind the cold rolling [operation 10], behind the precision work cold rolling [operation 12].
In addition, for the part beyond the above-mentioned part of mentioning, can with existing manufacture method in operation similarly carry out.
Although copper alloy plate of the present invention is preferably made by the manufacture method of above-mentioned embodiment, as long as but can obtain crystalline orientation in EBSD measures analyze in the cube orientation 001}＜100〉and area occupation ratio be 5～50% copper alloy plate, then above-mentioned [operation 1]～[operation 13] is not limited to and must sequentially carries out according to this, although be included in the above-mentioned method, but in above-mentioned [operation 1]～[operation 13], for example also can make by the method for as follows combination.
A. be following method: to the copper alloy starting material of the raw material that becomes copper alloy plate by casting [operation 1], thermal treatment [operation 2] homogenizes, hot-work [operation 3], water-cooled [operation 4], cutting [operation 5], cold rolling [operation 6], thermal treatment [operation 7], cold rolling [operation 8], middle solutionizing thermal treatment [operation 9], the order of cold rolling [operation 10] and Precipitation thermal treatment [operation 11] is implemented to process, wherein, described thermal treatment [operation 7] is 400～800 ℃ temperature, carry out in 5 seconds～20 hours the scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, and the working modulus R1 (%) in the described cold rolling [operation 10] is made as 5～65%.The requirement that the method can be applicable to intensity is not very strict situation.
B. be following method: to the copper alloy starting material of the raw material that becomes copper alloy plate by casting [operation 1], thermal treatment [operation 2] homogenizes, hot-work [operation 3], water-cooled [operation 4], cutting [operation 5], cold rolling [operation 6], thermal treatment [operation 7], cold rolling [operation 8], middle solutionizing thermal treatment [operation 9], Precipitation thermal treatment [operation 11], the order of precision work cold rolling [operation 12] and modified annealing [operation 13] is implemented to process, wherein, described thermal treatment [operation 7] is 400～800 ℃ temperature, carry out in 5 seconds～20 hours the scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, and the working modulus R2 (%) in the described precision work cold rolling [operation 12] is made as 5～65%.The same requirement that can be applicable to intensity with above-mentioned a. method of the method is not very strict situation.
C. be following method: to the copper alloy starting material of the raw material that becomes copper alloy plate by casting [operation 1], thermal treatment [operation 2] homogenizes, hot-work [operation 3], cutting [operation 5], cold rolling [operation 6], thermal treatment [operation 7], cold rolling [operation 8], middle solutionizing thermal treatment [operation 9], cold rolling [operation 10], Precipitation thermal treatment [operation 11], precision work cold rolling [operation 12], and the order of modified annealing [operation 13] is implemented to process, wherein, described thermal treatment [operation 7] is 400～800 ℃ temperature, carry out in 5 seconds～20 hours the scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, and with the working modulus R2 (%) in the working modulus R1 (%) in the described cold rolling [operation 10] and the described precision work cold rolling [operation 12] and be made as 5～65%.Temperature when the method can be applicable to hot-work [operation 3] end is the situation that does not need the temperature (for example, less than or equal to 550 ℃) of water-cooled [operation 4].
D. be following method: become copper alloy plate raw material the copper alloy starting material by the casting [operation 1], hot-work [operation 3], water-cooled [operation 4], cutting [operation 5], cold rolling [operation 6], thermal treatment [operation 7], cold rolling [operation 8], middle solutionizing thermal treatment [operation 9], cold rolling [operation 10], Precipitation thermal treatment [operation 11], precision work cold rolling [operation 12], and the order of modified annealing [operation 13] is implemented to process, wherein, described thermal treatment [operation 7] is 400～800 ℃ temperature, carry out in 5 seconds～20 hours the scope, described cold rolling [operation 8] carries out with the working modulus less than or equal to 50%, with the working modulus R2 (%) in the working modulus R1 (%) in the described cold rolling [operation 10] and the described precision work cold rolling [operation 12] and be made as 5～65%.The method can be applicable to that the slight situation of the segregation situation of casting in [operation 1] or segregation situation do not affect Cu alloy material and the situation of the electrical and electronic parts that gets by this Cu alloy material of processing.
Copper alloy plate of the present invention can be by satisfying foregoing, thereby satisfy for example desired characteristic of copper alloy for connector use sheet material.Especially, by the present invention can realize 0.2% endurance more than or equal to 600MPa, in 90 ° of W pliability tests of bendability flawless, and cut apart take thickness of slab flexible processing minimum bending radius value as less than or equal to 1, electric conductivity more than or equal to 35%IACS, stress relaxation-resistant characteristic less than or equal to 30% superperformance.
Embodiment
Below, based on embodiment the present invention is described in more details, but the present invention is not limited to these.
(embodiment 1)
Following alloy is dissolved by the high frequency melting furnace, and its speed of cooling with 0.1～100 ℃/second cast [operation 1], thereby obtained ingot bar, wherein, described alloy by shown in the composition on the alloying constituent hurdle of table 1 and table 2, allocating element like that so that comprise at least total amount be 0.5～5.0mass% be selected among Ni and the Co a kind or 2 kinds, comprise 0.3～1.5mass% Si, and the interpolation element that suitably contains other get, and remainder is comprised of Cu and inevitable impurity.This ingot bar is carried out 3 minutes to 10 hours the thermal treatment that homogenizes [operation 2] with 900～1020 ℃ temperature after, carry out hot-work [operation 3] (in the present embodiment, the beginning temperature is 900 ℃), then carry out shrend (being equivalent to water cooling [operation 4]), and in order to have carried out cutting [operation 5] except descaling.Afterwards, carry out the cold rolling [operation 6] of working modulus 80% to 99.8%, thermal treatment [operation 7] in 400 ℃～800 ℃ temperature and 5 seconds to 20 hours the scope, working modulus is 2%～50% cold rolling [operation 8], the middle solutionizing thermal treatment [operation 9] of 750 ℃～1020 ℃ temperature and 5 seconds～1 hour, working modulus is 3%～35% cold rolling [operation 10], the Precipitation thermal treatment [operation 11] of 400 ℃～700 ℃ temperature and 5 minutes～10 hours, working modulus is 3%～25% precision work cold rolling [operation 12], the sample of embodiment 1-1～1-19 and comparative example 1-1～1-8 has been made in the modified annealing [operation 13] of 200 ℃～600 ℃ temperature and 5 seconds～10 hours.Each thermal treatment and rolling after, carry out pickling or surface grinding according to the oxidation of material surface and the state of roughness, and correct by the tension force smoother according to shape.
Homogenize the suitable temperature and time of thermal treatment [operation 2] during according to the concentration of alloy and casting speed of cooling and difference.Therefore, adopted in the microtexture of ingot bar by observable dendritic being organized in through the basic temperature and time that disappears after the thermal treatment that homogenizes of the segregation of solute element.
Hot-work [operation 3] is carried out the material after the thermal treatment that homogenizes by common plastic working (rolling, extrude, withdrawing etc.).Temperature when hot-work begins is made as 600～1000 ℃ scope, so that material does not ftracture.
In addition, in each operation of the thermal treatment that homogenizes [operation 2], thermal treatment [operation 7], middle solutionizing thermal treatment [operation 9], Precipitation thermal treatment [operation 11], modified annealing [operation 13], carry out long thermal treatment during preferred low temperature, carry out the thermal treatment of short period of time during high temperature.The thermal treatment of low temperature and short period of time has the tendency that is difficult to show its effect, and high temperature and long thermal treatment have the tendency that produces the remarkable drawback that descends of intensity.
In addition, comparative example 1-5, the 1-6 in the following table do not carry out thermal treatment [operation 7] in the above-mentioned operation and cold rolling [operation 8] and makes.Comparative example 1-7,1-8 do not carry out the cold rolling [operation 10] in the above-mentioned operation, and have carried out precision work rolling [operation 12] with 3% working modulus.
For this sample, investigated following characteristic.Here, the thickness of sample is made as 0.15mm.In the result of the inventive example shown in the table 1, in the result of comparative example shown in the table 2.
The area occupation ratio of a.cube orientation and S orientation:
By the EBSD method, be 0.04～4mm measuring area
2, the scanning stride is to measure under the condition of 0.5～1 μ m.Measuring area adjusted take last crystal grain as benchmark to comprise 200.The scanning stride is adjusted according to crystal grain diameter, is during less than or equal to 15 μ m at average crystal grain diameter, carries out with 0.5 μ m stride, carries out with 1 μ m stride less than or equal to 30 μ m the time.The thermoelectron of the W filament of in the future self-scanning of electric wire electron microscope is as generating source.
B. bendability:
Vertically cut out the sample of width 10mm, length 35mm with rolling direction, the sample that will get so that the crooked axle mode vertical with rolling direction carried out the W bending this sample is as GW (Good Way), the sample that gets so that the crooked axle mode parallel with rolling direction carried out the W bending is made as BW (Bad Way), with 50 times observation by light microscope bend, investigated flawless.With the flawless O that is judged to be, will have being judged to be of crackle *.The angle of bend of each bend is made as 90 °, and the inner radius of each bend is made as 0.15mm.
C.0.2% endurance [YS]:
Be as the criterion with JIS Z2241 and measure 3 test pieces of JIS Z2201-13B number that cut out from rolling parallel direction, and show its mean value.
D: electric conductivity [EC]:
In the thermostatic bath that remains 20 ℃ (± 0.5 ℃), measure resistivity by four-terminal method, and calculated electric conductivity.In addition, terminal pitch is from being made as 100mm.
E: stress relaxation rate [SR]:
Take former days this electronic material industry can standard specifications (EMAS-3003) as standard, as shown below, under 150 ℃ * 1000 hours condition, measure.Loaded 80% initial stress of endurance by cantilever method.
Figure 1A, Figure 1B are the explanatory views of the test method of stress relaxation characteristics, and Figure 1A is the state before the thermal treatment, and Figure 1B is the state after the thermal treatment.Shown in Figure 1A, there is δ the position of the test piece 1 the when test piece 1 that keeps with cantilever on testing table 4 is applied 80% initial stress of endurance from benchmark
0Distance.It was kept 1000 hours in 150 ℃ thermostatic bath, and there is H the position of removing the test piece 2 behind the load from benchmark shown in Fig. 1 (b)
tDistance.Test piece when Reference numeral 3 is zero load, there is H its position from benchmark
1Distance.According to this relation, stress relaxation rate (%) is calculated and is (H
t-H
1)/δ
0* 100.
In addition, as same test method, also can adopt following method: as the technological standard scheme of Japan exhibition copper association (JCBA:Japan Copper and Brass Association: Japanese copper and brass association) " JCBAT309:2001 (temporarily); Stress relaxation test method based on the bending of copper and copper alloy thin plate bar "; " ASTM E328 as the test method of American Society for testing and materials (ASTM:American Society for Testing and Materials: U.S. test and materials association); Standard Test Methods for Stress Relaxation Tests for Materials and Structures: the standard test methods of the stress relaxation test of material and structure " etc.
Fig. 2 is based on above-mentioned JCBA T309:2001 (temporarily) and has utilized the bending deflection load of below deflection cantilever spiral formula with the explanatory view of the stress relaxation test method of test fixture.The principle of this test method is identical with the test method of the testing table that uses Fig. 1, so the value of stress relaxation rate also is essentially identical value.
In this test method, at first, test piece 11 is installed on the test fixture (testing apparatus) 12, at room temperature give predetermined displacement, keep removing load after 30 seconds, and with the bottom surface of test fixture 12 as reference plane 13, measured this face 13 with the distance of test piece 11 bending load points and as H
1Through after the scheduled time, from thermostatic bath or process furnace, take out at normal temperatures test fixture 12, unclamp for the screw 14 that loads deflection with unloading.After test piece 11 is cooled to normal temperature, the distance H between the flexural loads point of assay standard face 13 and test piece 11
tAfter the mensuration, revest bending deflection.In addition, in the drawings, the test piece during Reference numeral 11 expression unloading, the test piece when Reference numeral 15 expressions load deflection.Obtain permanent deflection displacement δ by following formula
t
δ
t＝H
i-H
t
According to this relation, calculating stress relaxation rate (%) is δ
t/ δ
0* 100.
In addition, δ
0Under the initial deflection displacement that obtains the required test piece of predetermined stress, by calculating with following formula.
δ
0＝σl
s 2/1.5Eh
Here, σ: the surperficial maximum stress (N/mm of test piece
2); H: thickness of slab (mm), E: flexibility factor (N/mm
2), l
s: span (mm).
The average crystal grain diameter [GS of cube grain] of the crystal grain of f.cube orientation:
By in the orientation analysis of EBSD, extract with respect to cube be oriented in ± 10 ° with interior orientation area, measure more than or equal to 20 crystal grain and calculated average.In addition, at this moment, the crystal grain inside of cube orientation and adjacency 221}＜212〉and be oriented to the twin crystal orientation that cube is orientated, also it is comprised in the cube orientation and analyzes.
Table 1
Table 2
As shown in table 1, inventive example 1-1～inventive example 1-19 bendability, endurance, electric conductivity, stress relaxation-resistant characteristic are all remarkable.But, as shown in table 2, when discontented foot regulation of the present invention, obtained the result of characteristic degradation.That is to say that comparative example 1-1 helps the precipitate of precipitation-hardening owing to the total amount of Ni and Co is rare density descends, thereby intensity is bad.In addition, do not form Si superfluous ground solid solution in metal structure of compound with Ni or Co, thereby electric conductivity is bad.Comparative example 1-2 is owing to the too much rate variance that conducts electricity of the total amount of Ni and Co.Comparative example 1-3 is intensity difference because Si is less.Comparative example 1-4 too much conducts electricity rate variance owing to Si.Bendability is poor because the ratio of cube orientation is few for comparative example 1-5 and comparative example 1-6.The Reduction by rolling behind the recrystallize is low owing to the ratio that improves the cube orientation for comparative example 1-7 and comparative example 1-8, its result, intensity difference.
(embodiment 2)
In the composition shown in the alloying constituent hurdle of table 3, for remainder by Cu and the inevitable copper alloy that forms of foreign material, make similarly to Example 1 the sample of the copper alloy plate of inventive example 2-1～2-17 and comparative example 2-1～2-3, and investigated similarly to Example 1 characteristic.In its result shown in the table 3.
Table 3
As shown in table 3, inventive example 2-1～inventive example 2-17 bendability, endurance, electric conductivity, stress relaxation-resistant characteristic are all remarkable.But, when discontented foot regulation of the present invention, characteristic is bad.That is to say that comparative example 2-1,2-2,2-3 are owing to the too much rate variance that conducts electricity of the addition of other elements.
(embodiment 3)
For with the copper alloy of the inventive example 2-11 same composition of table 3, except processing with working modulus, cold rolling [operation 10] and precision work cold rolling [operation 12] the working modulus R1 separately of the temperature and time of the thermal treatment shown in the table 4 [operation 7], cold rolling [operation 8] and the condition of R2, make similarly to Example 1 the sample of the copper alloy plate of inventive example 3-1～3-12 and comparative example 3-1～3-10, and investigated similarly to Example 1 characteristic.In its result shown in the table 4.In addition, in table 4, with simple must being designated as " [8] " such as " [operations 8] ", " precision work cold rolling [operation 12] " simple must being designated as " cold rolling [12] ".
Table 4
As shown in table 4, inventive example 3-1 is remarkable to inventive example 3-12 bendability, endurance, electric conductivity, stress relaxation-resistant characteristic.But, when discontented foot regulation of the present invention, characteristic is bad.That is to say, because the overlong time of the thermal treatment [operation 7] that the temperature of the thermal treatment of comparative example 3-1 [operation 7] is excessively low, excess Temperature, the comparative example 3-3 of the thermal treatment of comparative example 3-2 [operation 7] do not heat-treat [operation 7], comparative example 3-4, so the area occupation ratio of the orientation of cube separately descends, bendability worsens.Because it is too high that comparative example 3-5 does not carry out the working modulus of cold rolling [operation 8] of cold rolling [operation 8], comparative example 3-6, so the area occupation ratio of the orientation of cube separately descends, bendability worsens.Because the working modulus R1 of comparative example 3-7 and comparative example 3-8 and the summation of R2 are low, so intensity worsens.Because the working modulus R1 of comparative example 3-9 and comparative example 3-10 and the summation of R2 are high, so the area occupation ratio of cube orientation descends the bendability deterioration.
(embodiment 4)
About with the copper alloy of the inventive example 2-13 same composition of table 3, the example when finishing operation is made as timeliness thermal treatment [operation 11] is shown.Except processing with the condition of the working modulus R1 of the working modulus of the temperature and time of the thermal treatment shown in the table 5 [operation 7], cold rolling [operation 8], cold rolling [operation 10], make similarly to Example 1 the sample of the copper alloy plate of inventive example 4-1～4-2, and investigated similarly to Example 1 characteristic.In its result shown in the table 5.In addition, in table 5, " [operation 8] " etc. simply is designated as " [8] ", " precision work cold rolling [operation 12] " simply is designated as " cold rolling [12] ".
(embodiment 5)
About with the copper alloy of the inventive example 2-13 same composition of table 3, illustrate as the subsequent processing of middle solutionizing thermal treatment [operation 9] and example when having implemented Precipitation thermal treatment [operation 11].Except processing with the condition of the working modulus R2 of the working modulus of the temperature and time of the thermal treatment shown in the table 5 [operation 7], cold rolling [operation 8], precision work cold rolling [operation 12], make similarly to Example 1 the sample of the copper alloy plate of inventive example 5-1～5-2, and investigated similarly to Example 1 characteristic.In its result shown in the table 5.
(embodiment 6)
About with the copper alloy of the inventive example 2-11 same composition of table 3, illustrate as the subsequent processing of hot-work [operation 3] and example when having implemented cutting [operation 5].Except processing with working modulus, cold rolling [operation 10] and precision work cold rolling [operation 12] the working modulus R1 separately of the temperature and time of the thermal treatment shown in the table 5 [operation 7], cold rolling [operation 8] and the condition of R2, make similarly to Example 1 the sample of the copper alloy plate of inventive example 6-1～6-2, and investigated similarly to Example 1 characteristic.In its result shown in the table 5.In addition, in embodiment 6, the temperature when hot-work [operation 3] finishes all is set as 500 ℃.
(embodiment 7)
About with the copper alloy of the inventive example 2-11 same composition of table 3, the example when having implemented hot-work [operation 3] as the subsequent processing of casting [operation 1] is shown.Except processing with working modulus, cold rolling [operation 10] and precision work cold rolling [operation 12] the working modulus R1 separately of the temperature and time of the thermal treatment shown in the table 5 [operation 7], cold rolling [operation 8] and the condition of R2, make similarly to Example 1 the sample of the copper alloy plate of inventive example 7-1～7-2, and investigated similarly to Example 1 characteristic.In its result shown in the table 5.In addition, in embodiment 7, confirm the segregation situation of the ingot bar after casting [operation 1], and use the slight sample of segregation.In addition, the temperature during hot-work [operation 3] beginning is made as 900 ℃ similarly to Example 1, and has got started hot-work after ingot bar is heated to 900 ℃.
Table 5
As shown in table 5, inventive example 4-1, inventive example 4-2, inventive example 5-1 and inventive example 5-2 compare with inventive example 2-13, though find to have the tendency of endurance step-down, have enough characteristics as the copper alloy plate that is used for electrical and electronic parts.In addition, inventive example 6-1, inventive example 6-2, inventive example 7-1 and inventive example 7-2 compare with inventive example 2-11, have obtained in fact equal characteristic.
Though the present invention is illustrated based on embodiment, unless but we have special appointment, otherwise any details that our intention does not lie in explanation limits the present invention, and the present invention should can wide in rangely explain in the situation that does not break away from the invention spirit and scope shown in the application's claims.
The application require based on June 3rd, 2008 be the preference of Japanese JP2008-145707 at the application number that Japan proposes application for a patent for invention, its full content is herein incorporated as a part of content of this specification sheets record by reference.
Claims (17)
1. a copper alloy plate is characterized in that,
Have following composition: comprise any a kind or 2 kinds among Ni that total amount is 0.5～5.0mass% and the Co, and comprise the Si of 0.3～1.5mass%, and remainder is comprised of copper and inevitable impurity,
Yield strength σ 0.2 is more than or equal to 600MPa,
Electric conductivity is more than or equal to 35%IACS,
With the inside bend radius identical with thickness of slab, when the direction parallel with vertical with rolling direction carried out 90 ° of W bendings, flawless produced,
Load 80% stress of endurance, 150 ℃ of lower maintenances after 1000 hours,, stress relaxation rate is in 30%,
In the crystalline orientation that utilizes EBSD to measure is analyzed, the cube orientation 001}＜100〉and area occupation ratio be 7～47%.
2. copper alloy plate according to claim 1 is characterized in that, it comprises the Co of 0.5～2.0mass%.
3. copper alloy plate according to claim 1 and 2 is characterized in that,
Further, its S orientation 231}＜346〉and area occupation ratio be 5～40%.
4. copper alloy plate according to claim 1 and 2 is characterized in that,
Described copper alloy further contain total amount be 0.005～1.0mass% from the group who is formed by Sn, Zn, Ag, Mn, B, P, Mg, Cr, Fe, Ti, Zr and Hf, select at least a.
5. copper alloy plate according to claim 3 is characterized in that,
Described copper alloy further contain total amount be 0.005～1.0mass% from the group who is formed by Sn, Zn, Ag, Mn, B, P, Mg, Cr, Fe, Ti, Zr and Hf, select at least a.
6. according to claim 1,2 or 5 described copper alloy plates, it is characterized in that,
Cube orientation 001}＜100〉the average crystal grain diameter of crystal grain less than or equal to 17 μ m.
7. copper alloy plate according to claim 3 is characterized in that,
Cube orientation 001}＜100〉the average crystal grain diameter of crystal grain less than or equal to 17 μ m.
8. copper alloy plate according to claim 4 is characterized in that,
Cube orientation 001}＜100〉the average crystal grain diameter of crystal grain less than or equal to 17 μ m.
9. according to claim 1,2,5,7 or 8 described copper alloy plates, it is characterized in that described copper alloy contains the Co of 0.6～1.7mass%.
10. copper alloy plate according to claim 3 is characterized in that, described copper alloy contains the Co of 0.6～1.7mass%.
11. copper alloy plate according to claim 4 is characterized in that, described copper alloy contains the Co of 0.6～1.7mass%.
12. copper alloy plate according to claim 6 is characterized in that, described copper alloy contains the Co of 0.6～1.7mass%.
13. the manufacture method of a copper alloy plate for the manufacture of each described copper alloy plate in the claim 1 to 12, is characterized in that,
To the copper alloy starting material of the raw material that becomes described copper alloy plate by the casting as operation 1, the thermal treatment that homogenizes as operation 2, hot-work as operation 3, water cooling as operation 4, cutting as operation 5, cold rolling as operation 6, thermal treatment as operation 7, cold rolling as operation 8, middle solutionizing thermal treatment as operation 9, cold rolling as operation 10, Precipitation thermal treatment as operation 11, implement to process as the precision work cold rolling of operation 12 and as the order of the modified annealing of operation 13, described thermal treatment as operation 7 is 400～800 ℃ temperature, carry out in 5 seconds～20 hours the scope, described cold rolling as operation 8 carries out with the working modulus less than or equal to 50%, with described as the working modulus R1 in the cold rolling of operation 10 (%) with described as the working modulus R2 (%) in the precision work cold rolling of operation 12 and be made as 5～65%.
14. the manufacture method of copper alloy plate according to claim 13 is characterized in that,
With described Precipitation thermal treatment as operation 11, take this operation 11 as finishing operation, described thermal treatment as operation 7 is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling as operation 8 carries out with the working modulus less than or equal to 50%, is made as 5～65% with described as the working modulus R1 in the cold rolling of operation 10 (%).
15. the manufacture method of copper alloy plate according to claim 13 is characterized in that,
Implement described Precipitation thermal treatment as operation 11, take this operation 11 as the described heat treated subsequent processing of middle solutionizing as operation 9, described thermal treatment as operation 7 is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling as operation 8 carries out with the working modulus less than or equal to 50%, is made as 5～65% with described as the working modulus R2 (%) in the precision work cold rolling of operation 12.
16. the manufacture method of copper alloy plate according to claim 13 is characterized in that,
Implement described cutting as operation 5, take this operation 5 as described hot worked subsequent processing as operation 3, described thermal treatment as operation 7 is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling as operation 8 carries out with the working modulus less than or equal to 50%, with described as the working modulus R1 in the cold rolling of operation 10 (%) with described as the working modulus R2 (%) in the precision work cold rolling of operation 12 and be made as 5～65%.
17. the manufacture method of copper alloy plate according to claim 13 is characterized in that,
Implement described hot-work as operation 3, take the subsequent processing of this operation 3 as described casting as operation 1, described thermal treatment as operation 7 is carried out in 400～800 ℃ temperature, 5 seconds～20 hours scope, described cold rolling as operation 8 carries out with the working modulus less than or equal to 50%, with described as the working modulus R1 in the cold rolling of operation 10 (%) with described as the working modulus R2 (%) in the precision work cold rolling of operation 12 and be made as 5～65%.
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| JP2008145707 | 2008-06-03 | ||
| JP2008-145707 | 2008-06-03 | ||
| PCT/JP2009/060201 WO2009148101A1 (en) | 2008-06-03 | 2009-06-03 | Copper alloy sheet material and manufacturing method thereof |
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| JP7311651B1 (en) * | 2022-02-01 | 2023-07-19 | Ｊｘ金属株式会社 | Copper alloys for electronic materials and electronic parts |
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| JP3275377B2 (en) * | 1992-07-28 | 2002-04-15 | 三菱伸銅株式会社 | Cu alloy sheet with fine structure for electric and electronic parts |
| JP4809602B2 (en) | 2004-05-27 | 2011-11-09 | 古河電気工業株式会社 | Copper alloy |
| JP4584692B2 (en) * | 2004-11-30 | 2010-11-24 | 株式会社神戸製鋼所 | High-strength copper alloy sheet excellent in bending workability and manufacturing method thereof |
| JP4566048B2 (en) * | 2005-03-31 | 2010-10-20 | 株式会社神戸製鋼所 | High-strength copper alloy sheet excellent in bending workability and manufacturing method thereof |
| JP4254815B2 (en) * | 2006-06-21 | 2009-04-15 | 日立電線株式会社 | Copper alloy material for terminals and connectors |
| JP5028657B2 (en) | 2006-07-10 | 2012-09-19 | Ｄｏｗａメタルテック株式会社 | High-strength copper alloy sheet with little anisotropy and method for producing the same |
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2009
- 2009-06-03 CN CN200980128877.6A patent/CN102105610B/en active Active
- 2009-06-03 WO PCT/JP2009/060201 patent/WO2009148101A1/en active Application Filing
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2009148101A1 (en) | 2009-12-10 |
| JPWO2009148101A1 (en) | 2011-11-04 |
| US20110073221A1 (en) | 2011-03-31 |
| JP4875768B2 (en) | 2012-02-15 |
| CN102105610A (en) | 2011-06-22 |
| EP2298945A4 (en) | 2012-07-04 |
| EP2298945B1 (en) | 2014-08-20 |
| EP2298945A1 (en) | 2011-03-23 |
| US8641838B2 (en) | 2014-02-04 |
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